Annealing and Recrystallization

Materials Science 2- ENME 2421 January 31, 2014

Instructor: Maciej S. Kumosa

Author: Alisha Alomia Team Members: Gregg Gugegenheim, Matt Minuti, Luke Skelly

Introduction Deformations of certain materials are used to obtain desired dimensions and/or properties by applying stresses or heat treatment called annealing. Annealing is used to change the dislocation energy and the properties of the material. The annealing process consists of four different stages to change the microstructure of the material. The four stages are, cold work, recovery, recrystallization and grain growth. Cold work is when there has been not been any type of deformation performed on the material. Recovery is the softening of the material through the removal of primary dislocations and internal stresses. The recovery process occurs at lower temperatures and there is no appearance of strain free grains. Recrystallization is when strain free grains appear and begin to replace those that are deformed from internal stresses. Lastly, grain growth is when the microstructure begins to coarsen and the material may loose a substantial amount of its original strength. If the original strength is altered it can be recovered through hardening. The ductility, strength and hardness of the material change respectively with each stage in the annealing process. The most change is seen during recrystallization. The annealing process is typically done with varying temperatures, typically starting at 260 degrees Celsius and ending at 760 degrees Celsius. During the recrystallization process, a large decrease in the materials strength is seen while the ductility of the material increases. Procedure Four different samples of 70/30 brasses were used to compare crystal structures. The annealing temperatures of the samples of brass that were given were, not annealed, 380, 525 and 725 degrees Celsius respectively. The samples were first polished with #240, #400 and #600 sand paper, making sure the sand paper stayed damp while polishing. The specimen could not be rotated and an even pressure had to be applied constantly during the polishing process to ensure even polishing on the surface. When starting with a finer grit sandpaper, the brass had to

be positioned so that the new scratches would be perpendicular to the previous ones. The final step in the polishing process was polishing the brass with metcloth. Beuhler alpha polishing Alumina No.1 was poured onto the metcloth while polishing. The brass was then inserted into an ultrasonic cleaner for 3 minutes and followed by polishing again with the metcloth and gamma micropoish Alumina #3, following the same process done with the Alumina No. 1. While polishing with the metcloth, the scratches still had to be perpendicular to the previous ones. After polishing the brass the grains were exposed with an etching process using 45% Nitric Acid. The nitric acid allows the boundaries of the grains to corrode quickly while highlighting the edges. Only 80-95% nitric acid was available. The nitric acid was diluted using 4.8 mL of Nitric Acid and 10.67 mL of water. A high power optical microscope was used to capture the grains of the different specimens. A Rockwell hardening test was taken of each of the brass samples. Hardness was measured as a function of the ratio of the depth of penetration of the indenter due to the test load and the depth of penetration due to a minor pre-load. The B and C scales were used. Multiple were readings were taken to ensure accurate data. Results The results of the average hardness at each annealing temperature are listed below. The average was found by taking the average of the four trials. After looking at the microscopic pictures (Appendix: Figure 4, Figure 5, Figure 6, Figure 7) the average grain size was determined. The scale used in the pictures is 100 micrometers and 500 micrometers.

Table 1:

Hardness Testing (F-scale) Annealing Temperature Trial 1 Trial 2 Trial 3 Trial 4 Average Average grain size (micro meters) 20C 380C 525C 725C 67 55 33 21 67.5 57.5 35 24 67 57.5 36 24.5 67 57.5 35 24 67.125 56.875 34.75 23.375 25 50 30 250

Average Hardness at Annealing Temperature

80 70 60 Hardness 50 40 30 20 10 0 0 200 400 600 Annealing Temperature (C) 800 Series1

Figure 1: Average Hardness at Annealing Temperatures

Average Grain Size due to Annealing Temperature

300 Average Grain Size (micro meters) 250 200 150 Series1 100 50 0 20C 380C 525C Annealing Temperature (C) 725C

Figure 2: Average Grain Size Due To Annealing Temperature From the two plots above it can be seen that the recrystallization temperature is approximately 380 degrees Celsius. This can be determined because the hardness significantly changes at 380 degrees Celsius. The plateau before 380 degrees Celsius show that the material entered recrystallization after. It is seen in figure two as well because there is a slight peak at 380 degrees Celsius.

Discussion The results of the experiment are shown above in the two figures and table. Figure 1 shows a graphical relationship of the annealing temperature against the hardness of the material. Figure 2 shows a graphical relationship of the annealing temperature against the average grain size. Both tables show that the recrystallization stage begins at 380 degrees Celsius. When observing Figure one it can be seen that the recrystallization phase occurred starting around 380 degrees

and ending around 550 degrees Celsius. The new grains started to form only if the material was annealed at 380 degrees Celsius or above. Table 1 shows that while the hardness of the brass decreased, grain size increases. Both of the factors were measure by the use of hardness testing and the polishing and etching process to see the grains. Although figure one shows that grain growth begins around 550 and 600 degrees, it does not show when the annealing process ends. Further research would have to be done to see when there is no longer a change in the grain size. At that temperature is when the annealing process would be completely done. During this lab there were three main areas where sources of area could have arisen. The first source of error could have been that the samples of brass were not annealed correctly. There is no way to test that they were done correctly so assumptions had to be made that there was no error in the annealing process. Another source of error was not polishing and etching the samples correctly. Even with supervision of teaching assistants mistakes were still made. If pressed too hard the sample would have an uneven polish, causing there to not be a large enough area to see the grain sizes under the microscope. The last source of error could have been the hardness test. Although it was calibrated using samples with known errors, there were still variations in the hardness for each sample. Taking the average hardness of the samples did not give precise results unless many more samples were taken and the results were averaged. Conclusion In the experiment specific specimens of 70/30 brass were annealed at different temperatures that met the four stages of the annealing process. Hardness samples were taken from each of the samples to compare to the grain size of the samples. The grains size was found through the polishing and etching process. Tables and plots were made to show how the grain size, temperature and hardness were relative to each other. It can be seen that as the temperature increases, the hardness decreases and the grains size increases showing that the material becomes more ductile.

Executive Summary Four samples of brass were annealed at different temperatures, then polished and etched to observe the grain size. The samples were tested for hardness. The results showed the relationship between the annealing temperature, grain size, and the hardness of the material. It can be seen that as the hardness decreases, the temperature and grain size increase. References

"Annealing Review Heat Treatment - Engineers Edge." Annealing Review Heat Treatment - Engineers Edge. N.p., n.d. Web. 31 Jan. 2014. ENME 2421 Laboratory Manual Winter 2011

Appendix

Calculations: Assume 80%

Need 45% nitric acid from 80-95% source 6ml*0.8 = 4.8 ml nitric acid 4.8/.45 = 10.667 ml total 10.667 ml - 6 ml = 4.667 ml to add

Figure 3: Nitric Acid Calculations

Figure 4: Microscopic Pictures of Brass As Received

Figure 5: Microscopic Pictures of Brass Annealed at 380 Degrees Celsius

Figure 6: Microscopic Pictures of Brass Annealed at 525 Degrees Celsius

Figure 7: Microscopic Pictures of Brass Annealed at 725 Degrees Celsius